CN101826376B - Preparation method of vitrification substrate for radioactive nuclear waste - Google Patents

Preparation method of vitrification substrate for radioactive nuclear waste Download PDF

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CN101826376B
CN101826376B CN 201010164944 CN201010164944A CN101826376B CN 101826376 B CN101826376 B CN 101826376B CN 201010164944 CN201010164944 CN 201010164944 CN 201010164944 A CN201010164944 A CN 201010164944A CN 101826376 B CN101826376 B CN 101826376B
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raw material
temperature
waste matter
active nucleus
weight portions
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CN101826376A (en
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廖其龙
王辅
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Southwest University of Science and Technology
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Abstract

The invention relates to a preparation method of a vitrification substrate for radioactive nuclear wastes, which is characterized by comprising the following steps: mainly taking (NH4) H2PO4, Fe2O3 and H3BO3 as raw materials, proportioning, mixing, melting for 2-3.5 hours at the temperature of 1100-1250 DEG C, forming, and annealing, thereby preparing a vitrification body with glass of an iron-boron-phosphorus system as the substrate. The invention combines the advantages of high irradiation stability of the vitrification body of the borosilicate system and large waste-loading capacity of the vitrification body of the iron phosphate system. The prepared vitrification body has the advantages of excellent chemical stability and good thermal stability. Moreover, the invention has the advantages of simple preparation process and easy engineering, and can be widely applied in the curing treatment of radioactive nuclear wastes.

Description

A kind of preparation method who is used for active nucleus waste matter glass solidification base material
Technical field
The invention belongs to the method for handling the radioactive contamination material, relate to a kind of preparation method who is used for active nucleus waste matter glass solidification base material, be applicable to that the curing of the active nucleus waste matter that discharge in field such as nuclear industry is handled.
Background technology
Nuclear energy readjusts the energy structure, guarantees that to country energy security, propelling energy-saving and emission-reduction, reply climate change etc. have actively and profound significance as a kind of high-efficiency cleaning energy of technology comparative maturity.The history of existing over half a century of the peaceful use of nuclear energy has far-reaching influence to China and people of the world's growth in the living standard and progress of science and technology, has become the part that human pace of progress can not lack suddenly.But the development of nuclear cause unavoidably will produce nuclear waste, particularly in recent years and in the future a large amount of DECOMMISSIONING OF NUCLEAR FACILITIES, will produce a large amount of radioactive waste, especially high radioactivity nuclear waste (calls high-level waste in the following text).How it is handled safely and effectively and disposes, make it isolated with biosphere to greatest extent, become one of key issue that present domestic outer core career development needs to be resolved hurrily.
To active nucleus waste matter, present countries in the world are handled the comparison consensus to it and are: earlier radioactive waste is cured processing, will carries out the permanent geological disposal of deep layer after the firming body packing then.Wherein, solidifying processing is a vital step.The curing process of low-level waste and technology be comparative maturity, and has obtained the application of through engineering approaches.High-level waste solidify to be handled and to be mainly contained that artificial rock solidifies and two kinds of glass solidifications.Though it is all better that artificial rock solidifies geology stability, chemical stability, thermal stability and the anti-radiation property of handling firming body, but its curing process complexity, relatively poor with the compatibility that contains refuses such as high concentration sodium salt, selectivity to element in the high-level waste is very strong, and its technical requirement is very high, still is in the laboratory theoretical research stage at present; In addition, artificial rock solidifies the equipment complexity of using in the processing, the cost height, and the consumption of the material and the energy is all very big in the processing procedure.Therefore, countries in the world are glass solidifications to the preferred manner that high-level waste is cured processing at present.
In the prior art, the base material that is used for the glass solidification processing mainly contains borosilicic acid system glass and phosphate system glass.Borosilicate system glass is low because of melt temperature, chemical stability and irradiation stability are good, must be widely and use, but this system glass is to the non-constant of dissolubility of " objectionable impurities " in the refuse (as: phosphate, molybdate, sulfate, iron oxide and some other heavy metallic oxide), causes prepared firming body to be prone to " yellow phase " and performance does not reach requirement; Have to again before solidifying processing, nuclear waste be carried out pre-service for satisfying performance requirement, or by prolonging melting time, improving glass melting temperature, or be that cost reduces this type of " impurity " content in firming body to reduce the containing amount, aspect all is worthless improving volume reduction ratio and reduce cost etc. for this.And iron phosphate system glass has the ability that contains preferably to this type of " impurity ", and it is good to have chemical stability, and melt temperature is low and form characteristics such as adjustability is big, makes this system glass have original advantage as solidifying parent glass; But the relative borosilicate glass firming body with thermal stability of irradiation stability of iron phosphate system glass solidification body is relatively poor, and its practical application is restricted.
Summary of the invention
Purpose of the present invention is intended to overcome above-mentioned deficiency of the prior art, provide a kind of simple effectively, be the preparation method of the base material that is used for the active nucleus waste matter glass solidification of base material with iron boron phosphorus system glass, thereby provide a kind of new effective curing substrate for active nucleus waste matter solidifies to handle.
The present invention passes through at Fe 2O 3-P 2O 5Different in a different manner amounts add B in the system glass 2O 3Regulate melting technology, and analyze in conjunction with means such as scanning electron microscope (SEM) test, X-ray diffraction (XRD) test and chemically stable property testings, determine that a kind of is the active nucleus waste matter glass solidification disposal route of base material with iron boron phosphorus system glass.
Content of the present invention is: a kind of preparation method who is used for active nucleus waste matter glass solidification base material is characterized in that may further comprise the steps:
A, batching: mainly with component (NH 4) H 2PO 4(ammonium dihydrogen phosphate (ADP)), Fe 2O 3(iron oxide), H 3BO 3(boric acid) is raw material, and by (NH 4) H 2PO 445～75 weight portions, Fe 2O 315～35 weight portions, H 3BO 3The ratio of 5～15 weight portions is got each raw material;
B, mixing: each raw material is put into mixing apparatus mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2～3.5 hours under 1100 ℃～1250 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 700 ℃～850 ℃, is made article shaped;
E, annealing: article shaped placed under 400 ℃～500 ℃ the temperature and be incubated 1～2 hour, the rate of temperature fall with 0.5～1 ℃/min drops to room temperature then, promptly makes product.
In the content of the present invention: described step a batching can replace with: mainly with component P 2O 5(phosphorus pentoxide), Fe 2O 3, B 2O 3(boron oxide) is raw material, and presses P 2O 540～7.0 weight portions, Fe 2O 320～50 weight portions, B 2O 3The ratio of 4～15 weight portions is got each raw material.
In the content of the present invention: can also be added with Na in the described step a batching 2O (sodium oxide molybdena) and/or K 2O (kali), its adding proportion total amount is 2～15 weight portions.
In the content of the present invention: can also be added with CeO in the described step a batching 2(cerium oxide), its adding proportion are 3～15 weight portions.
In the content of the present invention: can also be added with active nucleus waste matter in the described step a batching, its adding proportion is 20～45 weight portions.
In the content of the present invention: heat described in the step c or/and melt cast described in the steps d is preferably under the stirring homogenizing and carries out.
In the content of the present invention: mixing apparatus described in the step b is can the ball milling mixing apparatus, also can be other mixing apparatus of the prior art.
In the content of the present invention: the component raw material described in the step a can also be can be decomposed into P under melt temperature 2O 5, Fe 2O 3, or/and B 2O 3, and do not introduce other starting material of impurity.
When the curing substrate that adopts the described method of content of the present invention to prepare is used for the active nucleus waste matter glass solidification, its solidification processing method is: directly active nucleus waste matter and the described batching of step a are fully mixed by charge ratio, fusion under glass melting temperature, after moulding and annealing, promptly making with iron boron phosphorus system glass is the active nucleus waste matter glass solidification body of base material again.
Compared with prior art, the present invention has following characteristics and beneficial effect:
(1) metallic ion can form the O-Me-O-P key (Me is mainly the Fe ion in the selected iron boron of the present invention phosphorus system glass in glass, also can be some other metal cation in the refuse), the O-Me-O-P key that forms has good stability, has strengthened the glass network structural stability.P elements all can exist with different group forms in the glass network structure with boron element simultaneously, and glass can reduce phosphorus oxygen network and boron oxygen network textural difference according to forming adjustment group form as far as possible and not be prone to phase-splitting; Therefore, the selected vitreum of the present invention system combines the better and iron phosphate system glass glass solidification body refuse bag advantage capacious of borosilicate system glass solidification body irradiation stability; The prepared active nucleus waste matter containing amount that goes out the glass solidification base material of the present invention reaches 30wt%;
(2) adopt the present invention, P elements is mainly with the very strong (P of water resisting property in the glass solidification body of preparation 2O 7) 4-The group form exists, and boron element is mainly with boron oxygen tetrahedron [BO 4] form exist, only contain few easily by aquation (PO 3) -The long-chain unit, have excellent chemical stability, and a better heat stability, 14 days mass loss rate＜10 in prepared 90 ℃ of deionized waters of firming body that go out -8Gcm -2Min -1
(3) preparation technology of the present invention is simple, and be easy to through engineering approaches and use, and cost is low, the production efficiency height, the curing that can be widely used in nuclear waste is handled, and operation is practical easily.
Embodiment
Embodiment given below intends so that the invention will be further described; but can not be interpreted as it is limiting the scope of the invention; the person skilled in art to some nonessential improvement and adjustment that the present invention makes, still belongs to protection scope of the present invention according to the content of the invention described above.
Embodiment 1:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component (NH 4) H 2PO 4, Fe 2O 3, H 3BO 3Be raw material, and by (NH 4) H 2PO 464g, Fe 2O 330g, H 3BO 36.5g ratio get each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) fully mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2.5～3 hours under 1150 ℃ temperature;
D, moulding: melt cast to being preheated to moulding in 850 ℃ the steel mold, is made article shaped;
E, annealing: article shaped placed under 450 ℃ the temperature insulation 1 hour, the rate of temperature fall with 1 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 2:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component (NH 4) H 2PO 4, Fe 2O 3, H 3BO 3, Na 2O is a raw material, and by (NH 4) H 2PO 456g, Fe 2O 326g, H 3BO 36g, Na 2The ratio of O12g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2.5～3 hours under 1150 ℃ temperature;
D, moulding: melt cast to being preheated to moulding in 800 ℃ the steel mold, is made article shaped;
E, annealing: article shaped placed under 450 ℃ the temperature insulation 1 hour, the rate of temperature fall with 1 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 3:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component (NH 4) H 2PO 4, Fe 2O 3, H 3BO 3, active nucleus waste matter is raw material, and by (NH 4) H 2PO 474g, Fe 2O 317g, H 3BO 3The ratio of 13g, active nucleus waste matter 30g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2.5～3 hours under 1200 ℃ temperature;
D, moulding: melt cast to being preheated to moulding in 800 ℃ the steel mold, is made article shaped;
E, annealing: article shaped placed under 450 ℃ the temperature insulation 1 hour, the rate of temperature fall with 1 ℃/min drops to room temperature then, promptly makes cured product.
Embodiment 4:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component (NH 4) H 2PO 4, Fe 2O 3, H 3BO 3Be raw material, and by (NH 4) H 2PO 445g, Fe 2O 315g, H 3BO 3The ratio of 5g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 3.5 hours under 1100 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 700 ℃, is made article shaped;
E, annealing: article shaped placed under 400 ℃ the temperature insulation 1 hour, the rate of temperature fall with 0.5 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 5:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component (NH 4) H 2PO 4, Fe 2O 3, H 3BO 3Be raw material, and by (NH 4) H 2PO 475g, Fe 2O 335g, H 3BO 3The ratio of 15g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 3.5 hours under 1250 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 850 ℃, is made article shaped;
E, annealing: article shaped placed under 500 ℃ the temperature insulation 2 hours, the rate of temperature fall with 1 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 6:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component (NH 4) H 2PO 4, Fe 2O 3, H 3BO 3Be raw material, and by (NH 4) H 2PO 455g, Fe 2O 325g, H 3BO 3The ratio of 10g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2.5 hours under 1200 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 780 ℃, is made article shaped;
E, annealing: article shaped placed under 450 ℃ the temperature insulation 1.5 hours, the rate of temperature fall with 0.8 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 7:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component P 2O 5, Fe 2O 3, B 2O 3Be raw material, and press P 2O 540g, Fe 2O 320g, B 2O 3The ratio of 4g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2 hours under 1100 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 700 ℃, is made article shaped;
E, annealing: article shaped placed under 400 ℃ the temperature insulation 1 hour, the rate of temperature fall with 0.5 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 8:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component P 2O 5, Fe 2O 3, B 2O 3Be raw material, and press P 2O 570g, Fe 2O 350g, B 2O 3The ratio of 15g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 3.5 hours under 1250 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 850 ℃, is made article shaped;
E, annealing: article shaped placed under 500 ℃ the temperature insulation 2 hours, the rate of temperature fall with 1 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 9:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component P 2O 5, Fe 2O 3, B 2O 3Be raw material, and press P 2O 550g, Fe 2O 340g weight portion, B 2O 3The ratio of 8g weight portion is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 3 hours under 1180 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 800 ℃, is made article shaped;
E, annealing: article shaped placed under 450 ℃ the temperature insulation 1.5 hours, the rate of temperature fall with 0.6 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 10:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component P 2O 5, Fe 2O 3, B 2O 3, CeO 2Be raw material, and press P 2O 560g, Fe 2O 340g, B 2O 310g, CeO 2The ratio of 6g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2.5 hours under 1200 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 750 ℃, is made article shaped;
E, annealing: article shaped placed under 460 ℃ the temperature insulation 1.3 hours, the rate of temperature fall with 0.7 ℃/min drops to room temperature then, promptly makes product---solidify parent glass.
Embodiment 11:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material may further comprise the steps:
A, batching: with component P 2O 5, Fe 2O 3, B 2O 3, active nucleus waste matter is raw material, and presses P 2O 550g, Fe 2O 330g, B 2O 3The ratio of 8g, active nucleus waste matter 20g is got each raw material;
B, mixing: each raw material is put into mixing apparatus (mortar or ball-grinding machine) mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2.5 hours under 1200 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 750 ℃, is made article shaped;
E, annealing: article shaped placed under 460 ℃ the temperature insulation 1.3 hours, the rate of temperature fall with 0.7 ℃/min drops to room temperature then, promptly makes cured product.
Embodiment 12-18:
A kind of preparation method who is used for active nucleus waste matter glass solidification base material, described material component of step a and proportioning (unit: restrain), the described melt temperature of step c see the following form:
Figure GSA00000110781200091
Other step, parameter are equal among the embodiment 1-11 arbitrary, slightly.
The invention is not restricted to the foregoing description, content of the present invention is described all can implement and have described good result.

Claims (3)

1. preparation method who is used for active nucleus waste matter glass solidification base material is characterized in that may further comprise the steps:
A, batching: mainly with component P 2O 5, Fe 2O 3, B 2O 3, active nucleus waste matter is raw material, and presses P 2O 540～70 weight portions, Fe 2O 320～50 weight portions, B 2O 3The ratio of 4～15 weight portions, active nucleus waste matter 20～45 weight portions is got each raw material;
Also be added with Na 2O and/or K 2O, its adding proportion total amount is 2～15 weight portions; Perhaps also be added with CeO 2, its adding proportion is 3～15 weight portions;
B, mixing: each raw material is put into mixing apparatus mix, make mixture;
C, fusion:, make melt with mixture heating and melting 2～3.5 hours under 1100 ℃～1250 ℃ temperature;
D, moulding: melt cast to the die for molding that is preheated to 700 ℃～850 ℃, is made article shaped;
E, annealing: article shaped placed under 400 ℃～500 ℃ the temperature and be incubated 1～2 hour, the rate of temperature fall with 0.5～1 ℃/min drops to room temperature then, promptly makes product.
2. by the described preparation method who is used for active nucleus waste matter glass solidification base material of claim 1, it is characterized in that: heating described in the step c is or/and melt cast described in the steps d is to carry out under the stirring homogenizing.
3. by the described preparation method who is used for active nucleus waste matter glass solidification base material of claim 1, it is characterized in that: mixing apparatus described in the step b is the ball milling mixing apparatus.
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